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Sodium hydride → HCID 19919792, 화합물

HRID 1648525
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HRID 1648525 반응식
[CH2:1]([C:5]1[N:6]([CH2:18][C:19]2[CH:28]=[CH:27][C:22]([C:23]([O:25][CH3:26])=[O:24])=[CH:21][CH:20]=2)[C:7](/[CH:10]=[C:11]2\[NH:12][C:13](=[O:17])[NH:14][C:15]\2=[O:16])=[CH:8][N:9]=1)[CH2:2][CH2:3][CH3:4].[H-].[Na+].[CH3:31][Si:32]([CH2:35][CH2:36][O:37][CH2:38]Cl)([CH3:34])[CH3:33]>CN(C=O)C>[CH2:1]([C:5]1[N:6]([CH2:18][C:19]2[CH:20]=[CH:21][C:22]([C:23]([O:25][CH3:26])=[O:24])=[CH:27][CH:28]=2)[C:7](/[CH:10]=[C:11]2\[NH:12][C:13](=[O:17])[N:14]([CH2:38][O:37][CH2:36][CH2:35][Si:32]([CH3:34])([CH3:33])[CH3:31])[C:15]\2=[O:16])=[CH:8][N:9]=1)[CH2:2][CH2:3][CH3:4]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 24758Sodium hydrideHCID 27242712-Chloromethyl 2-(trimethylsilyl)ethyl etherHCID 19086239methyl Z-4-[[2-butyl-5-[(2,5-dioxo-4-imidazolidinylidene)methyl]-1H-imidazol-1-yl]methyl]benzoate

생성물 1

HCID 19919792HCID 19919792, 화합물

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

To a solution of methyl Z-4-[[2-butyl-5-[(2,5-dioxo-4-imidazolidinylidene)methyl]-1H-imidazol-1-yl]methyl]benzoate (0.200 g, 0.524 mmol) in DMF (2 mL) is added sodium hydride (80% in oil, 0.02 g, 0.67 mmol) and the mixture stirred for 5 minutes. (Trimethylsilyl)ethoxymethyl chloride SEM-C1 (0.100 mL, 0.536 mmol) is added and the mixture allowed to stir for 16 hours. The solvents are removed in vacuo and the residue dissolved in ethyl acetate and water. After drying the organic fraction over MgSO4, the required product is isolated by chromatography, eluting with 0.5% methanol in chloroform. Crystallized from ether.

후처리

  1. addition(0.100 mL, 0.536 mmol) is added
  2. stirringto stir for 16 hours
  3. customThe solvents are removed in vacuo
  4. dissolutionthe residue dissolved in ethyl acetate
  5. dry with materialAfter drying the organic fraction over MgSO4

출처 및 근거

ORD 기록
ord-de845890a58c48fab02946360ff0c294
출처 데이터셋
uspto-grants-1995_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05436260

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